Process of producing nitrogen compounds.



A. R. FRANK. PROGESS OF PRODUCING NITROGEN GOMPOUNDS APPLIOATION PILED MAR. 23, 1908.* l 7 674 i Patented Mar. 21, 1911.

ame/Mo a Q fit"? %wa We t/meg a UT@ TATE@ PATENT lll hlltlll fo ALBERT EUDOLPH FRANK, or HALENsnE, NEAR BERLIN, GERMANY, ASSIGNOB TO THE FIRM or socmra GENERALE PER LA CIANAMIDE, or ROME, ITALY PROCESS OF PRODUCING NITROGEN COMPOUNDS.

Specification f Letters Patent.

Patented Mar. 21, 1 .911.

Original application filed March 13, 1907, Serial No. 362,()8& Divide& and this application filed March 23,'

CaC +2N:CaCN +C. This application is a division of ny former application Serial Number 362,()86, filed March 13, 1907.

Tn the production of nitrogen compounds' by the reaction of nitrogen with carbids, as for example, the ca'bids of the alkalies or alkaline earths, it has been ascertained that it is not necessary for the process that the entire mass of the carbid be brought to the temperature necessary for the reaction by supplying,` external or intrinsic heat to the entire mass; but that it sutlices if this temperature be produced at one place in the mass, when the rcaction thencontinues spontancously throughout the entire mass. A preliminary condition however is that the reaction temperature of from about 800 C. to 1100 C. be ,actually attained at this one place.

In accordance with the present invention the process may be carried ont in several ways, of which the following are iamples:

The ignition at one place may be produced by a convenient heating means evolving heat by Chemical reaction, which will 'aise the temperature at that place to the temperature required 'tor the conversion of the carbids, whereupon the Conversion will proceed spontaneously throughout the mass, sullicient nitrogen being present to eiect the conversion. The production of a tempe'a ture snfiiciently high for the absorption of nitrogen by the car-bid at one pla'ce or point of the carbid by means of said 'Chemical heating in order to raise the carhid at this one place to the proper ignition temperature may be acconplished-(c) by means of a primer comprisng an explosive mass or Serial No. 422,'779.

the likeg' or by means ofisubstances reacting with oarbid with the production of the necessary heat, which substances, if in the solid state suchas chlorate of potassiun, nitrate of alkali, etc., nay be added to the carbid at the place of ignition; while if the substances are gaseous, such as chlorin or oxygen, the same may be added to or employed with the first portions of the .nitrogen that are led to the carbid until the ignition has taken place; or (a) the requisite -tenperature may be produced by substances such as magnesium or aluminium which,

when 'mixed with the carbid at the place of ignition, react with the nitrogen with the production of the desired heat. ignition has produced a temperature sufiicent to cause a further absorption of the nitrogen, the latter is further supplied, and it will continue to be absorbed With a further development of heat so that the continued supply of nitrogen will cause the ab-' sorption to proceed spontaneously throughout the mass.

Referring to the accompanying drawing' After the j forning a part of this specification in which the figure reprcsents a diagrammatic sectional View of an apparatus suitable for carrying out my invention, l'represents a furnace or other suitable heating means; 2 a suitable container for the reacting substances; 3 an opening through which the said substances may be introduced; e an inlet fon the reacting gas, or gases; 5 an outlet for the same; and 6 an outlet for the finished product; it being, of course, 'understood that this apparatus merely illustrates one example of a meansby which the invention may be carried out. i u

Thefollowing example will explain how the present invention can be put into practice. For example, the heating by Chemical agencies may be accomplished by mining with the nitrogen such gases as will cause a local high temperature by reaction with the carbid, when the lattercis heated to emoderate temperature below the temperature of reaction. Such gases are oxygen, air, chlorin or the like. To carry out the process -by this means, a suitable proportion of such a gas is mixed with nitrogen and brought into reaction with the carbid, whereupon the temperature is raised to that required tor the Conversion, and s utficient nitrogen being supplied the reaction will continue without further heating until the entire mass is converted. Or, if desired, the temperature necessary for starting the reaetion may be obtained by the addition to the car-bid of substances such as powdered aluminiun or mag'esium, which will serve to start the reaction locally, and upon the nitrogen being supplied in proper quantity, the reaction will propagate itself throughout the entire mass. t

In carrying out the invention the Mitro geil may be supplied at a pressure equal to or above that of the atmosphere, or it may -be sucked into the receptacle at a pressure below that of the atmosphere.

The carbid may be used at any temperature below about 800 C. to 1,100 C., the temperature which isnecessary for the absorption of the nit-rogen; for the heat produced by such absorption will be suflicient to produce the reaction in the surrounding parts of the carbid. The nitrogen may be introduced at the ordinary temperature, or it may be heate d, while the e'arbid with which it is brought into contact, may be either cold or' warm. It is evident that .the higher the temperature of the reacting bodies (nitrogen or carbid) the easier and more quickly will 'the absorption of the nitrogen proceed. If carbid or nitrogen or both are employed in a warm stat-e, it is not necessary, according to the present invention, to heat these bodies to a temperature equal to or higher than the absorption temperature, since as has been shown by us, the heat produced by the absorption of the nitrogen itself, is suiicieht to cause the reaction to: proceed in and through the reacting mass. The progress of the raction, however, is accelerated by employing the nitrogen or the ca'bid or both at a temperature higher than the ordinary temperature, although the reacton proceeds without raising these bodies 'to an elevated temperature;

In all cases, there may be employed either pure or' commercial carbids, or -carbids mixed *with other materials, particularly with such materials as are adapted to facilitate or favorably influence the promotion of the absorption 'of the nitrogen, while ab sorption, as above stated, takes place according to the present invention through the heat produced by said absorption itself. Such other materials or additional substances may be e. g. cyanamid of calcium lime-nitrogen), oxids of alkaline earths or of other metals or salts thereof, such as chlorids, sulfates, sulds, or any suitable materials especially adapted to produce a loosening of the carbid mass. Carbonafeous materials are especially adapted'for this "purpose, because they by becoming carbonzed form :Channels or pores in the mass,

which ehannels or pores enable the introgen to penetrate easily throughout all the portions of the mass.

The carbid may be employed either in the powdered state or broken into lumps. Further, the carbid employed need not be completely formed carbid but may be in the form of its Components, as for example, a mixture of oxids and carbids or other salts of alkalies and alkaline earths and carbon or any carbonaceous substances derived from carbon; or as a mxture of metals and'car bon, or substances derived from carbon, with or without the addition of other organic or inorganic substances, provided these Components do not contain compounds having a temperature of decomposition which in itself or in reaction with the other Components is higher than the temperature of reaction when nitrogen acts on carbids.

It is to be clearly understood that the word carbid as used in this specification and in the claims, signifies and includes not only all pure carbids as such, but also carbids in the forms of their components, such as the mixture of oXids or other salts or metals with carbonaceous material, as indicated above. I

The nitrogen employed ma be either nitrogen as such or nitrogen ;p a combined state, such, for example, -as ammonia, provided the temperature at'which the nitrogen compound decomposes be lower thanthe temperature at which nitrogen reacts upon the carbid.

The nitrogen may be introduced into the carbid mass at the point where the absorption takes place, as above stated, and it may be further supplied in the direction in which this absorption proceeds, but the nitrogen may be also introduced i-n the opposite direction, so long as this gas passes through a portion of the mass which has not been acted upon or along the surface of the same toward the point where the absorption takes place. It is also to be'nderstood that the word ntrogen as used in this specification and in the claims specifies and includes not only pure nitrogen as such'but nitrogen mixed wth other gases, vapors or substances, as well as nitrogen in the combined state, such as ammonia, for example.

I am aware that .nitrogen compounds have hitherto bee`n produced from carbids by the reaction of ntrogen upon carbids and I therefore do not claim such method or process broadly, but

What I claim is 1. The process of making a compound of nitrogen by reacting upon-a carbid with nrrogen at a suitable temperature, whch consists in admixing with a portion of one of the reagents a substance eapable of chemaction, suppyng htrogen as the 'eacton proceeds, mantaning the temperztu'eand continuing the reacton throughout 'the mass to be converte.

.2. The process of making a compound of nt'ogen by reactng upon a oarbd With nit'ogen at a suitable temperature, which consists in mxing With a portion of the nitrogem 21 gas eapble of rez cting upon the car: bid to deveop heat sufficent to 'ntate 'the reaeton, supplyng ntrogen es the reaction p'oceeds, mantanng the temperature and oontnuing the reaoton throughout the mass to be converted;

3. The process of making a compound of nitrogen by reacting upon a, carbid wthnit-ogex &ta suitable temperature, which conssts in mxing oxygen with a portion of the ntrogen, supplying nitrogen as the reaoton prooees, mantairing the temperature and c'ontinung the reacton throughout themass to be converted.

?[n testmony that I claim the foregoing as my invention, I have signed my name' in presence of two subscrbing witnesses.

- ALBERT RUDOLPH'FRANK.

Wtneses:

HENRY HASPER, VOLDEMAR HAUPT. 

